CN105348149A - Method for improving quality of diphenylguanidine product - Google Patents
Method for improving quality of diphenylguanidine product Download PDFInfo
- Publication number
- CN105348149A CN105348149A CN201510933190.7A CN201510933190A CN105348149A CN 105348149 A CN105348149 A CN 105348149A CN 201510933190 A CN201510933190 A CN 201510933190A CN 105348149 A CN105348149 A CN 105348149A
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- CN
- China
- Prior art keywords
- product
- diphenylguanidine
- vulkacit
- thiambutosine
- quality
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C277/00—Preparation of guanidine or its derivatives, i.e. compounds containing the group, the singly-bound nitrogen atoms not being part of nitro or nitroso groups
- C07C277/08—Preparation of guanidine or its derivatives, i.e. compounds containing the group, the singly-bound nitrogen atoms not being part of nitro or nitroso groups of substituted guanidines
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to the technical field of diphenylguanidine production, and in particular discloses a method for improving the quality of a diphenylguanidine product. The method for improving the quality of the diphenylguanidine product takes diphenylthiourea as a raw material and is characterized by grinding the diphenylthiourea, throwing ammonium hydroxide and the diphenylthiourea into an oxidation pot according to the weight ratio being (7 to 10):1 for pulping, then pumping oxygen into the oxidation pot at the temperature of 55 to 85 DEG C, stopping oxygen pumping when a reaction reaches an end point, and then obtaining the diphenylguanidine product through washing and drying. The method provided by the invention is simple in step, convenient to operate, and easy to industrialize, the obtained product is white in appearance, and high in purity, the improvement of product quality is facilitated and the method is suitable for wide popularization and application.
Description
(1) technical field
The present invention relates to vulkacit D production technical field, particularly a kind of method improving vulkacit D quality product.
(2) background technology
Along with the development of society and the continuous propelling of technology, green tire and green manufacturing constantly connect, and the green tire in the current eye of people is not only the concept of " silicon tire ", but using all round process greenization of tire as strategic objective.Green tire is inseparable with the use of white carbon black (SiO2), and white carbon black, as the non-fossil supporting material of one, also has very important significance to the contribution of environment protection.And promotor vulkacit D obviously can accelerate the Silanization reaction of white carbon black and Si69, the Payne effect of system reduces, and improves the physical and mechanical properties of sizing material.
The development of green tire, also proposes higher requirement to the quality of vulkacit D.Compared with the promotor vulkacit D that existing Oxygen Catalytic Oxidation method technique and the method for lead oxide or sodium cyanide method are produced, color and luster is partially yellow or partially grey, and purity is on the low side.
(3) summary of the invention
The present invention, in order to make up the deficiencies in the prior art, provides a kind of simple, the method for the raising vulkacit D quality product that product appearance is pure white, purity is high.
The present invention is achieved through the following technical solutions:
A kind of method improving vulkacit D quality product, take thiambutosine as raw material, it is characterized in that: thiambutosine is pulverized, the weight ratio that ammoniacal liquor and thiambutosine press 7-10:1 drops in stills for air blowing and pulls an oar, then at 55-85 DEG C, logical oxygen in stills for air blowing, stops logical oxygen, then obtains vulkacit D product through washing, drying when reaction is reached home.
More excellent scheme of the present invention is:
Described thiambutosine pulverizes rear mistake 100 mesh sieve, obtains evengranular fine and closely woven thiambutosine.
The mass concentration of described ammoniacal liquor is 16-20%.
Step of the present invention is simple, and easy to operate, be easy to industrialization, the product appearance obtained is pure white, and purity is high, is convenient to the quality product improving product, is suitable for wide popularization and application.
(4) embodiment
Embodiment 1:
700g ammoniacal liquor is dropped in stills for air blowing, ammonia concn 16%, 100g grinds, thiambutosine after sieving, opens and stirs, after making beating 30min, by heating material to 60 DEG C, in stills for air blowing, pass into oxygen, stop logical oxygen when reaction is reached home, through the finished product washed, drying is promoted agent vulkacit D.Promotor vulkacit D white appearance, purity reaches 98.0%.
Embodiment 2:
800g ammoniacal liquor is dropped in stills for air blowing, ammonia concn 18%, 100g grinds, thiambutosine after sieving, opens and stirs, after making beating 30min, by heating material to 70 DEG C, in stills for air blowing, pass into oxygen, stop logical oxygen when reaction is reached home, through the finished product washed, drying is promoted agent vulkacit D.Promotor vulkacit D white appearance, purity reaches 98.6%.
Embodiment 3:
900g ammoniacal liquor is dropped in stills for air blowing, ammonia concn 20%, 100g grinds, thiambutosine after sieving, opens and stirs, after making beating 30min, by heating material to 80 DEG C, in stills for air blowing, pass into oxygen, stop logical oxygen when reaction is reached home, through the finished product washed, drying is promoted agent vulkacit D.Promotor vulkacit D white appearance, purity reaches 99.0%.
Claims (3)
1. one kind is improved the method for vulkacit D quality product, take thiambutosine as raw material, it is characterized in that: thiambutosine is pulverized, the weight ratio that ammoniacal liquor and thiambutosine press 7-10:1 drops in stills for air blowing and pulls an oar, then at 55-85 DEG C, logical oxygen in stills for air blowing, stops logical oxygen, then obtains vulkacit D product through washing, drying when reaction is reached home.
2. the method for raising vulkacit D quality product according to claim 1, is characterized in that: described thiambutosine pulverizes rear mistake 100 mesh sieve.
3. the method for raising vulkacit D quality product according to claim 1, is characterized in that: the mass concentration of described ammoniacal liquor is 16-20%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510933190.7A CN105348149A (en) | 2015-12-15 | 2015-12-15 | Method for improving quality of diphenylguanidine product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510933190.7A CN105348149A (en) | 2015-12-15 | 2015-12-15 | Method for improving quality of diphenylguanidine product |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105348149A true CN105348149A (en) | 2016-02-24 |
Family
ID=55324236
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510933190.7A Pending CN105348149A (en) | 2015-12-15 | 2015-12-15 | Method for improving quality of diphenylguanidine product |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105348149A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106631907A (en) * | 2016-10-14 | 2017-05-10 | 山东尚舜化工有限公司 | Synthetic rubber accelerator system and technique |
| CN106810469A (en) * | 2017-02-24 | 2017-06-09 | 山东尚舜化工有限公司 | The device and its production method of a kind of continuous production thiofide diphenylguanidine |
| CN108727228A (en) * | 2017-10-23 | 2018-11-02 | 科迈化工股份有限公司 | A kind of vulcanization accelerator diphenylguanidine（DPG）Continuous production processes |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4898978A (en) * | 1985-01-17 | 1990-02-06 | Akzo N.V. | Process for the preparation of N,N'-disubstituted guanidines |
| CN1057832A (en) * | 1990-06-29 | 1992-01-15 | 沈阳化工学院 | Preparation technique of diphenyl guanidine |
| SK2012004A3 (en) * | 2004-05-03 | 2005-11-03 | Vucht, A. S. | Method for the production of N,N'-disubstituted guanidines |
| CN102358727A (en) * | 2011-08-29 | 2012-02-22 | 科迈化工股份有限公司 | Method for synthesizing rubber vulcanization promoter diphenylguanidine by mother liquor use |
| CN102363601A (en) * | 2011-09-20 | 2012-02-29 | 科迈化工股份有限公司 | Method for producing rubber accelerator DGP by using hydrogen peroxide as oxidant |
-
2015
- 2015-12-15 CN CN201510933190.7A patent/CN105348149A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4898978A (en) * | 1985-01-17 | 1990-02-06 | Akzo N.V. | Process for the preparation of N,N'-disubstituted guanidines |
| CN1057832A (en) * | 1990-06-29 | 1992-01-15 | 沈阳化工学院 | Preparation technique of diphenyl guanidine |
| SK2012004A3 (en) * | 2004-05-03 | 2005-11-03 | Vucht, A. S. | Method for the production of N,N'-disubstituted guanidines |
| CN102358727A (en) * | 2011-08-29 | 2012-02-22 | 科迈化工股份有限公司 | Method for synthesizing rubber vulcanization promoter diphenylguanidine by mother liquor use |
| CN102363601A (en) * | 2011-09-20 | 2012-02-29 | 科迈化工股份有限公司 | Method for producing rubber accelerator DGP by using hydrogen peroxide as oxidant |
Non-Patent Citations (2)
| Title |
|---|
| 岐雨涝等: "二苯胍合成技术进展", 《河北化工》 * |
| 施涵青等: "橡胶促进剂二苯胍生产方法的研究", 《化学世界》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106631907A (en) * | 2016-10-14 | 2017-05-10 | 山东尚舜化工有限公司 | Synthetic rubber accelerator system and technique |
| CN106810469A (en) * | 2017-02-24 | 2017-06-09 | 山东尚舜化工有限公司 | The device and its production method of a kind of continuous production thiofide diphenylguanidine |
| CN106810469B (en) * | 2017-02-24 | 2019-09-24 | 山东尚舜化工有限公司 | A kind of device and its production method of continuous production thiofide diphenylguanidine |
| CN108727228A (en) * | 2017-10-23 | 2018-11-02 | 科迈化工股份有限公司 | A kind of vulcanization accelerator diphenylguanidine（DPG）Continuous production processes |
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Application publication date: 20160224 |
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| RJ01 | Rejection of invention patent application after publication |